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The crystal structure of the title compound, [Re(C8H6N4)(CO)3(H2O)]PF6·2H2O, shows the Re center to be in a distorted octa­hedral geometry with a facial distribution of the carbonyl ligands. Two other water mol­ecules are hydrogen bonded to the coordinated water mol­ecule. The cation lies on a crystallographic mirror plane, across which the anion is disordered.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807017734/hk2150sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536807017734/hk2150Isup2.hkl
Contains datablock I

CCDC reference: 647235

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](C-C) = 0.004 Å
  • Disorder in solvent or counterion
  • R factor = 0.016
  • wR factor = 0.037
  • Data-to-parameter ratio = 11.6

checkCIF/PLATON results

No syntax errors found



Alert level A DIFF019_ALERT_1_A _diffrn_standards_number is missing Number of standards used in measurement. DIFF020_ALERT_1_A _diffrn_standards_interval_count and _diffrn_standards_interval_time are missing. Number of measurements between standards or time (min) between standards. DIFF022_ALERT_1_A _diffrn_standards_decay_% is missing Percentage decrease in standards intensity.
Alert level C PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT125_ALERT_4_C No _symmetry_space_group_name_Hall Given ....... ? PLAT243_ALERT_4_C High 'Solvent' Ueq as Compared to Neighbors for F3 PLAT243_ALERT_4_C High 'Solvent' Ueq as Compared to Neighbors for F4 PLAT243_ALERT_4_C High 'Solvent' Ueq as Compared to Neighbors for F6 PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for P2 PLAT250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor .... 2.22 PLAT302_ALERT_4_C Anion/Solvent Disorder ......................... 33.00 Perc. PLAT431_ALERT_2_C Short Inter HL..A Contact F6 .. O1 .. 2.98 Ang. PLAT480_ALERT_4_C Long H...A H-Bond Reported H102 .. O1 .. 2.62 Ang. PLAT751_ALERT_4_C Bond Calc 0.97000, Rep 0.9713(16) ...... Senseless su O3 -H103 1.555 1.555 PLAT751_ALERT_4_C Bond Calc 0.91000, Rep 0.910(2) ...... Senseless su O101 -H101 1.555 1.555 PLAT751_ALERT_4_C Bond Calc 0.93000, Rep 0.932(3) ...... Senseless su O101 -H102 1.555 1.555 PLAT752_ALERT_4_C Angle Calc 117.00, Rep 117.07(15) ...... Senseless su RE1 -O3 -H103 1.555 1.555 1.555 PLAT752_ALERT_4_C Angle Calc 97.00, Rep 97.2(2) ...... Senseless su H101 -O101 -H102 1.555 1.555 1.555 PLAT755_ALERT_4_C D-H Calc 0.91000, Rep 0.910(2) ...... Senseless su O101 -H101 1.555 1.555 PLAT755_ALERT_4_C D-H Calc 0.93000, Rep 0.933(3) ...... Senseless su O101 -H102 1.555 1.555 PLAT755_ALERT_4_C D-H Calc 0.93000, Rep 0.933(3) ...... Senseless su O101 -H102 1.555 1.555 PLAT755_ALERT_4_C D-H Calc 0.93000, Rep 0.933(3) ...... Senseless su O101 -H102 1.555 1.555 PLAT755_ALERT_4_C D-H Calc 0.97000, Rep 0.9710(17) ...... Senseless su O3 -H103 1.555 1.555 PLAT756_ALERT_4_C H...A Calc 1.99000, Rep 1.994(3) ...... Senseless su H101 -N2 1.555 2.655 PLAT756_ALERT_4_C H...A Calc 2.62000, Rep 2.622(2) ...... Senseless su H102 -O1 1.555 2.654 PLAT756_ALERT_4_C H...A Calc 1.67000, Rep 1.670(2) ...... Senseless su H103 -O101 1.555 6.657
Alert level G PLAT199_ALERT_1_G Check the Reported _cell_measurement_temperature 293 K
3 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 23 ALERT level C = Check and explain 1 ALERT level G = General alerts; check 5 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 2 ALERT type 2 Indicator that the structure model may be wrong or deficient 0 ALERT type 3 Indicator that the structure quality may be low 20 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check

Computing details top

Data collection: APEX2 (Bruker, 2006); cell refinement: APEX2; data reduction: SAINT (Bruker, 2006); program(s) used to solve structure: SHELXTL (Bruker, 2006); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.

fac-Aqua(bipyrazine)tricarbonylrhenium(I) hexafluorophosphate dihydrate top
Crystal data top
[Re(C8H6N4)(CO)3(H2O)]PF6·2H2ODx = 2.258 Mg m3
Mr = 627.42Mo Kα radiation, λ = 0.71073 Å
Orthorhombic, PnmaCell parameters from 8341 reflections
a = 15.5869 (6) Åθ = 3.0–43.0°
b = 13.1068 (5) ŵ = 6.77 mm1
c = 9.0349 (4) ÅT = 293 K
V = 1845.78 (13) Å3Block, orange
Z = 40.42 × 0.24 × 0.20 mm
F(000) = 1192
Data collection top
Bruker Kappa-APEXII
diffractometer
1892 independent reflections
Radiation source: fine-focus sealed tube1880 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.034
φ and ω scansθmax = 26.0°, θmin = 3.5°
Absorption correction: numerical
(SADABS; Bruker, 2006)
h = 1919
Tmin = 0.158, Tmax = 0.450k = 1616
49927 measured reflectionsl = 1111
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.016Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.037H-atom parameters constrained
S = 1.17 w = 1/[σ2(Fo2) + (0.0071P)2 + 4.7736P]
where P = (Fo2 + 2Fc2)/3
1892 reflections(Δ/σ)max = 0.001
163 parametersΔρmax = 0.68 e Å3
0 restraintsΔρmin = 0.67 e Å3
Special details top

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
C10.82905 (17)0.1471 (2)0.9631 (3)0.0246 (6)
C20.7097 (3)0.25000.8145 (5)0.0273 (9)
C30.84846 (19)0.0471 (2)0.6279 (3)0.0265 (6)
H30.82910.01410.71260.032*
C40.8740 (2)0.0096 (2)0.5074 (4)0.0310 (7)
H40.87140.08030.51310.037*
C50.9042 (2)0.1350 (2)0.3794 (3)0.0294 (6)
H50.92350.16740.29410.035*
C60.87832 (17)0.1940 (2)0.4986 (3)0.0228 (6)
O10.82694 (15)0.08427 (18)1.0518 (3)0.0374 (5)
O20.6365 (2)0.25000.8250 (4)0.0411 (8)
O30.96933 (17)0.25000.7918 (3)0.0238 (6)
O1010.52257 (16)0.06874 (17)0.6314 (3)0.0370 (5)
N10.85100 (14)0.14918 (18)0.6248 (3)0.0207 (5)
N20.90248 (18)0.0332 (2)0.3828 (3)0.0324 (6)
P20.63555 (8)0.25000.32697 (12)0.0302 (2)
F10.6022 (3)0.25000.1613 (4)0.0858 (14)
F20.6640 (3)0.25000.4909 (4)0.108 (2)
F30.5475 (4)0.2138 (7)0.3846 (7)0.110 (5)0.50
F40.6768 (9)0.1465 (6)0.3355 (10)0.126 (4)0.50
F50.5921 (6)0.1392 (5)0.3165 (7)0.0808 (19)0.50
F60.7203 (4)0.2023 (8)0.2657 (9)0.120 (5)0.50
Re10.832360 (9)0.25000.812157 (16)0.01747 (6)
H1010.55410.03370.69920.072 (15)*
H1020.56250.06650.55460.12 (2)*
H1030.99950.18970.82640.048 (11)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
C10.0204 (13)0.0302 (15)0.0231 (14)0.0001 (11)0.0008 (11)0.0023 (12)
C20.025 (2)0.032 (2)0.025 (2)0.0000.0035 (17)0.000
C30.0326 (15)0.0201 (14)0.0268 (14)0.0033 (12)0.0013 (12)0.0007 (12)
C40.0394 (17)0.0204 (14)0.0333 (16)0.0014 (13)0.0031 (14)0.0039 (12)
C50.0386 (16)0.0277 (15)0.0220 (14)0.0007 (13)0.0012 (13)0.0016 (12)
C60.0253 (13)0.0216 (14)0.0214 (13)0.0020 (11)0.0023 (11)0.0001 (11)
O10.0425 (13)0.0387 (13)0.0309 (12)0.0003 (10)0.0033 (10)0.0149 (11)
O20.0200 (16)0.061 (2)0.0424 (19)0.0000.0024 (14)0.000
O30.0198 (13)0.0218 (14)0.0298 (15)0.0000.0012 (11)0.000
O1010.0499 (14)0.0261 (11)0.0351 (12)0.0097 (10)0.0081 (11)0.0008 (10)
N10.0211 (11)0.0192 (11)0.0218 (11)0.0011 (9)0.0028 (9)0.0003 (9)
N20.0434 (15)0.0254 (13)0.0284 (13)0.0031 (12)0.0010 (12)0.0084 (11)
P20.0395 (6)0.0285 (6)0.0225 (5)0.0000.0007 (5)0.000
F10.100 (3)0.127 (4)0.0311 (18)0.0000.0110 (19)0.000
F20.086 (3)0.206 (6)0.033 (2)0.0000.021 (2)0.000
F30.071 (3)0.194 (14)0.066 (3)0.068 (5)0.000 (3)0.062 (5)
F40.215 (12)0.053 (4)0.109 (7)0.079 (6)0.035 (7)0.031 (4)
F50.113 (6)0.049 (3)0.080 (4)0.023 (4)0.019 (4)0.015 (3)
F60.057 (3)0.220 (15)0.082 (5)0.059 (5)0.007 (3)0.025 (6)
Re10.01705 (8)0.01873 (8)0.01662 (8)0.0000.00096 (5)0.000
Geometric parameters (Å, º) top
C1—O11.150 (4)O101—H1010.910 (2)
C1—Re11.918 (3)O101—H1020.932 (3)
C2—O21.145 (5)N1—Re12.167 (2)
C2—Re11.912 (4)P2—F4i1.503 (6)
C3—N11.338 (4)P2—F41.503 (6)
C3—C41.377 (4)P2—F3i1.543 (5)
C3—H30.930P2—F31.543 (5)
C4—N21.334 (4)P2—F21.546 (4)
C4—H40.930P2—F61.563 (6)
C5—N21.334 (4)P2—F6i1.563 (6)
C5—C61.386 (4)P2—F11.585 (4)
C5—H50.930P2—F51.606 (6)
C6—N11.351 (4)P2—F5i1.606 (6)
C6—C6i1.468 (5)Re1—C1i1.918 (3)
O3—Re12.143 (3)Re1—N1i2.167 (2)
O3—H1030.9713 (16)
O1—C1—Re1178.9 (3)F3—P2—F6i174.1 (5)
O2—C2—Re1175.9 (4)F2—P2—F6i95.6 (3)
N1—C3—C4121.0 (3)F3i—P2—F191.5 (3)
N1—C3—H3119.5F3—P2—F191.5 (3)
C4—C3—H3119.5F2—P2—F1177.5 (3)
N2—C4—C3122.4 (3)F6—P2—F186.7 (3)
N2—C4—H4118.8F6i—P2—F186.7 (3)
C3—C4—H4118.8F4i—P2—F5179.4 (7)
N2—C5—C6122.3 (3)F3i—P2—F585.6 (5)
N2—C5—H5118.9F6—P2—F588.5 (5)
C6—C5—H5118.9F4—P2—F5i179.4 (7)
N1—C6—C5120.3 (3)F3—P2—F5i85.6 (5)
N1—C6—C6i115.78 (15)F6i—P2—F5i88.5 (5)
C5—C6—C6i123.92 (17)C2—Re1—C1i88.01 (12)
Re1—O3—H103117.07 (15)C2—Re1—C188.01 (12)
H101—O101—H10297.2 (2)C1i—Re1—C189.30 (17)
C3—N1—C6117.5 (3)C2—Re1—O3175.71 (15)
C3—N1—Re1126.1 (2)C1i—Re1—O395.03 (10)
C6—N1—Re1115.85 (18)C1—Re1—O395.03 (10)
C4—N2—C5116.5 (3)C2—Re1—N198.20 (12)
F4i—P2—F3i94.9 (6)C1i—Re1—N1170.92 (10)
F4—P2—F394.9 (6)C1—Re1—N197.49 (11)
F3i—P2—F286.1 (3)O3—Re1—N178.43 (8)
F3—P2—F286.1 (3)C2—Re1—N1i98.20 (12)
F4i—P2—F691.0 (8)C1i—Re1—N1i97.49 (11)
F3i—P2—F6174.1 (5)C1—Re1—N1i170.92 (10)
F2—P2—F695.6 (3)O3—Re1—N1i78.43 (8)
F4—P2—F6i91.0 (8)N1—Re1—N1i75.14 (12)
Symmetry code: (i) x, y+1/2, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O101—H101···N2ii0.910 (2)1.994 (3)2.882 (4)164.83 (18)
O101—H102···F50.933 (3)2.395 (7)3.180 (8)141.7 (3)
O101—H102···F30.933 (3)2.475 (7)2.955 (7)112.1 (2)
O101—H102···O1iii0.933 (3)2.622 (2)3.168 (3)117.99 (15)
O3—H103···O101iv0.9710 (17)1.670 (2)2.611 (3)161.87 (17)
Symmetry codes: (ii) x+3/2, y, z+1/2; (iii) x+3/2, y, z1/2; (iv) x+1/2, y, z+3/2.
Re—O and O···O distances (Å) top
CompoundRe—OO···O
(I)2.143 (3)2.611 (3)
(II)2.1902.623
(III)2.181
 

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